Reactive fluid transfer apparatus



June 29, 1965 H. L. HACKETT 4 REACTIVE FLUID TRANSFER APPARATUS Filed Nov. 24, 1961 2 Sheets-Sheet l IIIIIIII' FIG. 4

INVENTOR.

HOMER L. HAG/(E T T ATTORNE Y June 29, 1965 H. L. HACKETT 3,191,640

REACTIVE FLUID TRANSFER APPARATUS Filed Nov. 24, 19 61 2 Sheets-Sheet 2 INVENTOR.

HOMER L. HACKETT United States Patent O 3,191,640 REACTEVE FLUID TRANSFER APPARATUS Homer L. Hackett, Ponca City, Okla, assignor to Continental Oil Company, Penca City, Okla, a corporation of Delaware Filed Nov. 24, 1961, Ser. No. 154,702 8 Claims. ((31. 141-63) This invention relates to apparatus for transferring reactive liquids from one container to another.

Prior to this invention, the devices for transferring reactive liquids have been, for the most part, extremely complicated and complex. One device, known as the dry box, is large and cumbersome, made of metal and extremely difiicult to Work within. Access to the interior of the box is generally provided by a pair of rubber gloves that attach to the outside and extend within the box. Other forms of transfer boxes have been constructed of canvas to reduce the weight but still require the use of cumbersome rubber gloves. While the canvas box does provide a more portable unit and does provide more visibility than the metal-type box, it still suffers from the inherent difliculty of being cumbersome and difiicult to use and operate. Another prior art device provides for the transfer of liquids from one bottle to another through the use of concentric hypodermic needles. All of these devices, however, are rather difiicult to use and, for the most part, cumbersome in operation. None of the above-mentioned apparatuses is convenient for the transfer of reactive liquids from one bottle to another in an inert atmosphere, nor is any of the apparatuses easy to use, simple and economical to construct and build, and readily. adaptable to practically any size bottle or container.

It is an object of this invention, therefore, to provide a device that will permit the transfer of a reactive fluid from one container to a second container within an inert atmosphere, which is simple to build and economical to construct.

It is a further object of this invention to provide a device for transferring liquids from one container to a second in an inert atmosphere that is readily adaptable to various type bottle sizes. i

It is a further object of this invention to provide a device for preventing spilled chemicals from seeping into the containers, thereby causing them to become contaminated.

It is a still further object of this invention to provide a device for purging the various bottles prior to the transfer of the liquid so that all traces of atmosphere will be removed, thereby eliminating oxidation or contamination of the reactant mixture by oxidation.

In accordance with one embodiment of my invention, a box is provided with a slidably mounted top lid. The bottom, or side opposite the slidable lid, has a plurality of openings transverse therethrough. Each opening has an annular gasket mounted on the outside of the lid and about the opening. An opening is placed centrally in the upper slidable lid and opposite the holes in the body of the box. The jars containing the solutions to be transferred and the jar that the solution is to be transferred to, are held against the gaskets. The interior of both the box and the bottles is purged of air by forcing an inert atmosphere into the transfer box. In order to transfer liquid from a bottle to a second bottle, a hypodermic needle or other suitable device is pushed through the opening in the top or lid of the box and into the interior of the box. The lid is slid until the hypodermic needle is directly above the annular opening between the interior of the box and the bottle containing the solution to be transferred. The needle is then lowered into the solution to be transferred and the plunger pulled until a sufficient amount of solution is within the hypodermic. The

3,191,640 Patented June 29, 1965 "ice hypodermic needle is then withdrawn from the bottle. The hypodermic and lid are then slid over the second bottle and the hypodermic needle again lowered into the interior of the empty bottle wherein the hypodermic plunger is depressed until the solution is emptied within the bottle.

Other objects and advantages of this invention will become apparent from the following description and claims when read in view of the accompanying drawings, in which:

'FIG. 1 is the side view of this invention, showing the hypodermic needle inserted within the box and a plurality of bottles pressed against the gaskets in the lower portion of the liquid transfer device;

FIG. 2 is a top view of the transfer apparatus;

FIG. 3 is a cross-sectional view of a portion of another embodiment of this invention showing a method for purging the individual bottles and also shows the dam provided around the openings through the bottom of the box used to prevent spilled fluid from entering the bottles;

FIG. 4 is a cross-sectional end view of a portion of the transfer apparatus;

FIG. 5 is a cross-sectional view of a circular transfer apparatus taken through 5--5 in FIG. 6; and

FIG. 6 is the top view of a circular transfer apparatus.

Referring to the figures in general, and in particular to FIGS. 1 and 2, an embodiment of the invention is shown wherein a box generally referred to as 10 has a bottom 11, and a plurality of sides 12, 13, 14 and 15. A top 16 is slidably mounted on box 10 and retained thereon by a plurality of L-shaped guides 17 and 18. The guides are attached to side 15 by means such as screws or rivets 19, or by any other suitable method such as by gluing. At the bottom 11 of box 10 is a plurality of openings 20a, 2% and 20c which permit communication between the interior of box It and a plurality of bottles or flasks 21a, 21b and 21c suspended therebelow. Each bottle, for example, 21a, has associated with it a gasket 22a which permits a tight seal between the bottom 11 of box 10 and the bottle 21a. In order to securely press the bottle against the gasket, a suitable support such as a corresponding plurality of ringstand supports 23a, can be provided.

In lieu of this type of support, an annular elastic member, for example, can be substituted for the gasket which has an opening capable of accepting a bottle and secureiy holding it therein. It is obvious to one skilled in the art that other forms of retaining means can obviously be employed to hold flask 21a in substantially air-tight relationship with the interior of box Iii.

The top 16 of box 10 is likewise provided with an opening 25 which is adapted to permit the insertion of a hypodermic needle 27 of a hypodermic 28. Tightly surrounding hypodermic needle 27 is a gasket 26 which likewise forms a substantially air-tight seal around needle 27. Lid 16 is likewise provided with extensions 16a and 16b for the purpose of maintaining a tight cover over box 10 when hypodermic needle 27 is moved over the mouth of the bottles when liquids are transferred from one to the other. high-pressure tank 40 which is controlled by a valve 41. A tube or other conveying means 42 is used to convey the inert gas to box 10. An opening 30 which can be placed at any convenient location in box 10 is, in this particular embodiment, placed through side 13. A rubber seal or grommet 31 is used to substantially provide an airhight seal.

OPERATION The operation of the device is fairly simple. Hpyodermic 23 has its needle 27 inserted through gasket 26 and The inert gas supply can consist of a cylindrical opening 25 of lid 16 into the interior of box 10. A plurality of bottles or flasks 21a, 21b and 210 is tightly secured to the bottom of the box and sealed against gaskets 22a, 22b and 220, respectively. Pressure contact is afforded the flasks against their respective seals by means of ringstand supports 23a, 23b and 23c, respectively. Any of the three flasks shown in this particular embodiment may contain a fluid that is to be transfer-red to the other. Preferably, a fluid 34 to be tranferred, is placed in the center jar 21b. Prior to the transfer of any fluids, valve 41 is opened and an inert gas under pressure leaves tank 40 and travels through tube 42 to the interior of box 10. While any inert gas may be used, argon is preferred since it is heavier than air, a characteristic that will provide easy purging of the bottles, since the weight of the argon will completely supplant the air within the bottle. For ease of operation, the bottles may usually have the stoppers removed prior to mounting them in the equipment since the defusion of air-into the openings of the bottles will normally be relatively slow. After the bottles are mounted, suflicient time is allowed for the inert gas to purge all traces of air from the interior of both box and flasks 21a, 21b and 21c. This may take several minutes. Once the air has been satisfactorily removed, the fluids are ready to be transferred from one container or flask to the other. If, for example, the fluid to be transferred is contained in flask 21]), the hypodermic needle 27 is inserted into the mouth of flask 21b and plunger 29 is withdrawn moving the fluid up the hypodermic needle and into the barrel of the hypodermic. The hypodermic needle is then withdrawn from the jar and pulled up sufliciently into the interior of box 10. The hypodermic needle is then moved, sliding lid 16 until the hypodermicneedle is axial with the opening of the flask, for example 21a, in which the fluid is to be transferred. The hypodermic needle is then lowered through the opening 20a, until theneedle is within the mouth of the flask. Plunger 29 is then depressed forcing the fluid from hypodermic 28, down needle 27 and into flask 21a. If, for example, flasks 21a and 21b both contain fluids that are to be mixed in 210, hypodermic 28 is moved until it is over the mouth of flask 20a. The needle is then inserted into 21a and the fluids drawn into the hypodermic 28. Hypodermic is then removed and the entire lid slid down until the hypodermic is over the opening of flask 21c. Hypodermic is then pushed down, placing the needle within 210 and plunger 29 is depressed, forcing the fluid from the hypodermic 28 into the interior of the flask. The same procedure would be followed with flask 2111, thus, depositing both fluids into flask 210.

It is obvious that less bottles may be used by stoppering the openings from the bottom 11 of box 10 and likewise more bottles may be used by providing more openings through base 11. It is also obvious that more hypodermics can be used by providing additional openings in top 16. An additional length L1 may necessarily have to be added in order to prevent uncovering the interior of box 10 for the location of the new hypodermic.

FIG. 3 shows a method for providing an easy purge for a bottle such as, for example, 21a. In this embodimerit, a L-shaped tube 50 is inserted through hole 30 of grommet 31 and has tube 42 connected thereto. Argon is then passed through tube 42, L-shaped tube 50 and into the interior of bottle 21a. When the bottle is sufficiently purged, the L-shaped tube is moved from position a to position b, thereby providing a methodof purging the interior of the box 10. The stem 51 of L-shaped tube 50 is made sufliciently long so it can reach the openings b or 20c (see FIG. 1) by sliding 50 over the holes and then lowering them into the mouth of the bottles.

FIG. 3 also shows a dam 60 which provides a slight raise around the opening 20a in bottom 11. This generally will prevent any spilled liquid from accidentally flowing into the container and thereby causing contamination of the container.

FIG. 4 is a side view illustrating another form of the invention, and also illustrating another method of securing the flask over the holes 20a. Gasket 22, rather than being an annular ring as shown in FIGS. 1, 2 and 3, comprises an elastic collar and has an opening adapted to forcibly accept bottle 21, providing a substantially airtight seal. The opening 20a may also be made larger in order to facilitate a stopper 61 which is especially useful in the case of extremely reactive solutions. Thus, the bottle 21a may be pressed into the gasket and the entire system purged of air by inert gas.

An eye is mounted in the top of stopper 61 in order to facilitate the removal of said stopper from bottle 21. A rod 63, having a hook 64 on one end thereof may be placed through hypodermic hole 25 and the rod and lid moved until the hook 64 engages the eyelet 65. An upward movement of the rod will then disengage the stopper 61 from bottle 21. The stopper may be placed inside box 10 beside the opening 20a until the transfer of liquid is complete. The stopper may then be replaced in the same manner as it was removed.

Referring to FIGS. 5 and 6, a circular, reactive-fluid transfer apparatus is shown. A circular base 11 has mounted about its circumference a perpendicular wall 70. Evenly spaced about the circumference of the base is a plurality of holes 8t which are similar in construction to the holes 26 in the base 11 of the transfer mechanism shown in FIG. 1. Below the holes are similarly located washers 82, bottle 81 and ringstand support 83 for bottle 81. Bottles 84 and 85 have similar Washers and ringstand supports. This embodiment also has a top 42 which conveys the inert gas through a washer 31 mounted in opening 36 to the internal portion of the transfer apparatus. Hole 25 similarly contains a washer 26 which is adapted to receive a hypodermic needle 27. A slot 53 is adapted to slidably receive a lid 58 which is cross hatched to indicate plastic, but may, for example, be made out of glass or other transparent material. The operation of this embodiment is similar to that described in conjunction with FIGS. 1-4 except that lid 53 is rotated in order to place hypodermic needle 27 over the respective jars 81-85 rather than being slid over the various jars as described in the operation of FIG. 1. This embodiment presents several advantages: first, the lid does not require the lengthy extensions 16a and 16b required for lid 16; and, second, the system is adaptable for receiving a larger number of jars since they can be easily mounted about the circumference of the base 11. It is obvious also that a combination of FIGS. 1 and 6 could be made. This combination would provide several rows of bottles about the'base 11 shown in FIGS. 5 and 6. In order for the hypodermic to move from one row to the other, it could he slid as is shown in FIG. 1. Bottles in the same row could be reached by rotating lid 58 as is shown in FIG. 5.

Applicant has explained one embodiment of this invention. It is obvious that other embodiments, improvements, modifications and changesmay be made that are well within the scope of the invention herein described and shown. For example, the material used to construct the box can be made of Plexiglas, other plastics, either transparent or opaque, metal or glass. It is, of course, obvious that some visible opening is desirable since it would facilitate operation of the device. Likewise, other forms of purging gases and other methods of clamping the bottles to the box could quite easily be provided in lieu of those particularly shown and described by applicant. While the preferred embodiment of the invention shows a slidable lid, it is obvious to those skilled in the art that a rigid lid could be used if it is provided with a plurality of openings above each of the flasks. A bottle,

for example, 210, may also be included which contains a solvent for washing the hypodermic.

Examples of how the embodiments are actually used are hereinafter given.

Example I Referring to the drawing shown in FIG. 1, prior to the insertion of bottles 21a, 21b'or 21c, valve 41 was opened and inert gas from cylinder 45) was permitted to flow into transfer apparatus until all of the air was'expelled from the apparatus. A bottle 21a, which contained triethyl aluminum, was unstopped and pressed against gasket 22a and the ringstand base 23a was moved up against the bottom of the bottle so that it wassecurely .pressed against the gasket. The sample botle 2112 was likewise pressed up against gasket 22b and secured by ringstand 23b. Air was then expelled from each of the bottles by normal turbulence of the incoming inert atmosphere. The procedure may be hastened by using L-shaped probe 59 to force the air from the bottle. The needle of hypodermic 28 was then inserted into the hole through the lid and into bottle 21a. Aluminum triethyl was then expelled from the hypodermic needle.

Example 11 A bottle containing titanium tetrachloride in solution with kerosene was desired to be mixed with triethyl aluminum. Using the design shown in FIGS. 5 and 6, the transfer apparatus was flushed of air of inert gas through pipe 42. The bottle that will contain the mixed solution was applied over a hole, for example, 82, and flushed of air. The stoppers from the titanium tetrachloride container and the triethyl aluminum container were then removed and the bottles placed over addi tional holes in base 11 similar to 89. Using the design in FIG. 6, a fourth bottle containing a hypodermic cleaning solution was included. In order to mix the solution, the hypodermic needle 27 was lowered into one of the two solutions, for example, titanium tetrachloride. The hypodermic was then filled with the required amount of solution, removed from the bottle and centered over the bottle that was to receive the mixture. The hypodermic needle was then lowered and the solution expelled from the hypodermic. In order to prevent contamination of the triethyl aluminum by the titanium tetrachloride remaining in the hypodermic, the hypodermic was cleaned, using the cleaning solution by lowering hypodermic needle 27 into the cleaning solution and rinsed several times. The needle was then removed from the cleaning solution and lowered into the triethyl aluminum which was then pulled up into the hypodermic needle 27 and in like manner, transferred over the bottle that had the titanium tetrachloride transferred thereto. The hypodermic needle was then lowered into the container and depressed thereby expelling the solution and completing the mixture of the two chemicals.

It is, therefore, to be understood that all matter herein set forth or shown in the accompanying drawings is to be interpreted as illustrative and not in a limiting sense. Having described my invention, I claim as new and desire to secure by Letters Patent:

1. A device for permitting the transfer of fluids in an inert atmosphere by means of a hypodermic and hypodermic needle, said device comprising: a container having a bottom and sides; a plurality of openings provided through the bottom of said container; a plurality of corresponding gaskets below said plurality of openings; means for communicating an inert atmosphere into the interior of said container; a cover slidably mounted on the top of said container and forming a substantially air-tight seal for the interior thereof, said cover having an opening therethrough and adapted to permit the insertion of said hypodermic needle, the cover additionally including extensions having a length sufi'icient to permit movement of said cover without exposing the interior of 6 said container to the atmosphere during said movement. 2. A device for permitting the transfer of fluids in an inert atmosphere by means of a hypodermic and hypodermic needle, said device comprising: a container having a bottom and sides, said bottom having at least two openings therethrough, said openings additionally ha ing corresponding gaskets mounted thereabout; an additional opening through said container; inert gas means, said inert gas means communicated through said third opening and into the interior of said container; a slidable cover for said container, said cover adapted to substantially render said container air-tight, said cover additionally including extensions thereto having a length sunrcient to permit longitudinal movement of said cover without causing the interior of said container to be exposed to the atmosphere; a fourth opening through said cover, said fourth opening adapted to permit the insertion of said hypodermic needle therethrough, whereby said hypodermic needle may be slidably moved above either said first or second openings.

3. A device for permitting the transfer of fluids in an inert atmosphere, said device comprising: a container defined by a bottom, first and second sides, and first and second ends, said bottom having a plurality of openings therethrough, each of said openings having a corresponding annular ring-type gasket mounted thereabout on the external side of said bottom; a plurality of bottle mounting means adjacent each of said plurality of openings and adapted to securely confine a bottle below each of said openings and tightly against said annular ring gaskets; means for communicating an inert atmosphere into said container; a cover for said container slidably mounted on the opposite side of said bottom and engaging the sides and ends of said container, said top additionally including extensions, said extensions having sufficient lengths to permit said top to slide without causing exposure of the internal portion of said container to the atmosphere, said top addi tionally including an opening adapted to permit a hypodermic needle to pass therethrough, said opening opposite the plurality of openings through the bottom of said container, the opening in the top and the plurality of openings in the bottom of said container adapted to permit a hypodermic needle to pass through the openings in the top of said container and selectively pass through the openings in the bottom of said container and into a jar con fined therebelow.

4. A device as described in claim 3 wherein said means for permitting inert atmosphere to enter the internal portion of said container comprises an L-shaped tube; a source of inert atmosphere; means to communicate said source to said L-shaped tube, said L-shaped tube being tentatively mounted within said container and adapted to permit said inert atmosphere to be selectively directed through the openings in the bottom of said container and into a jar confined therebelow, then into the interior of said container.

5. A device for permitting the transfer of fluids in an inert atmosphere employing a hypodermic needle comprising: a container having bottom, sides and a top, said bottom having at least two openings therethrough, said openings additionally having corresponding gaskets mounted thereabout on the external side of said bottom; means for communicating inert gas into the interior of said container; and means in the lid of said container for permitting the insertion of a hypodermic needle into said container and over the openings in the bottom of said container.

sponding gaskets mounted thereabout on the external side of said bottom; means for communicating inert gas into the interior of said container and means in the lid of said container for permitting the insertion of said hypodermic needle into said container and over the openings in the bottom of said container whereby a hypodermic needle when inserted through the opening in the top of said container may be further'inserted into a jar containing a reactive fluid mounted over one of the openings in the bottom of said container and when the needleis withdrawn it may be repositioned over another hole in'the bottom of said container by applying pressure to said lid causing said'lid to slidably rotate.

8. A device as described in claim 6 wherein the top of said container is made of .a rigid transparent plastic.

References Cited by the Examiner UNITED STATES PATENTS 997,881 7/11 Weintraub 23-259 XR 0 2,355,260 8/44 Bower et al 141-130 XR 2,382,696 8/45 De Milleville 1416 2,566,430 9/51 Sobers 23259 2,584,397 2/52 Pitman 14159 FOREIGN PATENTS v569,649 1/59 Canada.

References Cited by the Applicant UNITED STATES PATENTS 2,192,140 2/40 McCreary. 2,756,129 7/56 Harris. 2,786,740 3/57 Taylor et a1.

LAVERNE D. GEIGER, Primary Examiner.

LOUIS J. DEMBO, Examiner. 

1. A DEVICE FOR PERMITTING THE TRANSFER OF FLUIDS IN AN INERT ATMOSPHERE BY MEANS OF A HYPODERMIC AND HYPODERMIC NEEDLE, SAID DEVICE COMPRISING: A CONTAINER HAVING A BOTTOM AND SIDES; A PLURALITY OF OPENINGS PROVIDED THROUGH THE BOTTOM OF SAID CONTAINER; A PLURALITY OF CORRESPONDING GASKETS BELOW SAID PLURALITY OF OPENINGS; MEANS FOR COMMUNICATING AT INERT ATMOSPHERE INTO THE INTERIOR OF SAID CONTAINER; A COVER SLIDABLY MOUNTED ON THE TOP OF SAID CONTAINER AND FORMING A SUBSTANTIALLY AIR-TIGHT SEAL FOR THE INTERIOR THEREOF, SAID COVER HAVING AN OPENING THERETHROUGH AND ADAPTED TO PERMIT THE INSERTION OF SAID HYPODERMIC NEEDLE, THE COVER ADDITIONALLY INCLUDING EXTENSIONS HAVING A LENGTH SUFFICIENT TO PERMIT MOVEMENT OF SAID COVER WITHOUT EXPOSING THE INTERIOR OF SAID CONTAINER TO THE ATMOSPHERE DURING SAID MOVEMENT. 